CN103881320A - Nanometer flame-retardant polybutylene telephthalate material and preparation method thereof - Google Patents
Nanometer flame-retardant polybutylene telephthalate material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nanometer flame-retardant polybutylene telephthalate material and a preparation method thereof. The nanometer flame-retardant polybutylene telephthalate material disclosed by the invention comprises, by mass, 30 to 60% of polybutylene telephthalate, 15 to 30% of a reinforcing agent, 10 to 20% of a compound fire retardant, 5 to 10% of a flexibilizer, 3 to 5% of a compatilizer, 0.1 to 0.5% of a surface treating agent, 0.1 to 1% of a lubricating agent and 0.1 to 1% of an anti-oxidant.
Description
Technical field
The present invention relates to a kind of technical field of polymer materials, specifically a kind of nano flame retardant polybutylene terephthalate material and preparation method thereof.
Background technology
Polybutylene terephthalate (PBT) is the linear saturated polyester resin of a kind of crystal type, the industries such as electronic apparatus, household electrical appliances, automotive industry are widely used in, but these industries have strict requirement to burning, safety performance, so add fire retardant to improve its flame retardant resistance and to guarantee the aspect such as safety in utilization of product in PBT, become an important topic to PBT research and development in recent years.In PBT, adding effective fire retardant is one of effective, the most most economical means that improve at present flame retardant resistance.It is several that the most frequently used fire retardant mainly contains halogen, P-N type, silicon-type class and inorganic nano class etc.In combustion processes, can generate a large amount of cigarette and poisonous for halogen fire retardant, gas is corrosive, environment is caused to serious pollution, therefore, P-N type, the fire retardant of silicon-type class and inorganic nano class becomes the parent that environment-friendly health type fire retardant is subject to people gradually and looks at, particularly since 21 century, the generally popularization of nanotechnology, nano material is considered to the most promising material of 21 century, and the research boom that become international, therefore preparation interpolation nano-meter flame retardants is one of important method obtaining the polybutylene terephthalate material with high flame resistance.
Summary of the invention
The object of the present invention is to provide a kind of good heat resistance, intensity high and there is nano flame retardant polybutylene terephthalate material of superior electrical performance and preparation method thereof.
The technical solution adopted for the present invention to solve the technical problems is: nano flame retardant polybutylene terephthalate material, its component by mass percent proportioning is: polybutylene terephthalate 30%～60%, toughener 15%～30%, compound flame redundant 10%～20%, toughner 5%～10%, compatilizer 3%～5%, surface treatment agent 0.1%～0.5%, lubricant 0.1%～1%, oxidation inhibitor 0.1%～1%.
Described toughener is the one in alkali free glass fibre, nano-calcium carbonate, nano kaoline, wollastonite, whisker.
Described compound flame redundant is the compound that nano-sized magnesium hydroxide 30wt%, nano imvite 20wt% and polysilane fire retardant 50wt% three mix, wherein all silane modified processing of nano-sized magnesium hydroxide and nano imvite.
Described toughner is the one in acrylonitrile-butadiene-styrene copolymer (ABS), ethylene-vinyl acetate copolymer (EVA), MBS (MBS).
Described compatilizer is the one in ethylene-methyl acrylate-glyceryl methacrylate terpolymer (E-MA-GMA), maleic anhydride grafted ethene-propylene-non-conjugated diene hydrocarbon copolymer (EPDM-g-MAH), maleic anhydride extension bar ethylene-octene copolymer (POE-g-MAH), maleic anhydride graft styrene-butadiene-styrene (SBS-g-MAH).
Described surface treatment agent is the one in Magnesium Stearate, titanic acid ester, Aluminate, silane and phosphoric acid ester.
Described lubricant is calcium stearate or ethylene bis stearic amide.
Described oxidation inhibitor is the compound of hindered phenol antioxygen 1076 and phosphite ester kind antioxidant 168.
The preparation method of above-mentioned nano flame retardant polybutylene terephthalate material, comprises the following steps:
(1) polybutylene terephthalate is dried to 3～5 hours at 130 ℃～140 ℃, moisture control is below 0.03%, stand-by;
(2) toughener is dried to 3～6 hours at 80 ℃～110 ℃, take by weight ratio more dried toughener and surface treatment agent, add together in the high-speed mixer of 3000～8000 revs/min, at the temperature that maintains 80 ℃～110 ℃, stir 10～60 minutes, make evenly coated toughener of surface treatment agent, then be cooled to and make surface-treated toughener lower than 40 ℃, stand-by;
(3) take by weight ratio nano imvite 20wt% and the polysilane fire retardant 50wt% of the nano-sized magnesium hydroxide 30wt% of silane modified processing, silane modified processing, make to mix, make compound flame redundant, then at 80 ℃～85 ℃, be dried 30～45 minutes, stand-by;
(4) take by weight ratio polybutylene terephthalate, compound flame redundant and the surface treated toughener after drying treatment, after mixing, add again the toughner, compatilizer, lubricant and the oxidation inhibitor that take by weight ratio, then add together in high-speed mixer and fully mix 10～30 minutes;
(5) material again step (4) being mixed adds and in twin screw extruder, carries out abundant fusion plastification and mediate mixing, melt temperature is controlled at 190 ℃～250 ℃, after extruding by twin screw extruder, obtain nano flame retardant polybutylene terephthalate material of the present invention through overcooling, pelletizing, after dry.
The invention has the beneficial effects as follows, the present invention is combined nanotechnology with macromolecular material, the nano flame retardant polybutylene terephthalate material that utilizes the compound flame redundant of nano modification and polybutylene terephthalate melt blending and make by twin-screw extrusion, there is the excellent flame retardancy energy that Halogen presses down cigarette, reach UL94V-0 flame retardant grade, and drip phenomenon without melting in combustion processes, its product also has good gloss simultaneously, dimensional stabilizing, low warpage, high-modulus, high heat-resisting, the performances such as high impact-resistant, and cost is low, can be widely used in electric, automotive industry, the fields such as mechanical fitting, have a extensive future.
Embodiment
Further illustrate technical scheme of the present invention below in conjunction with specific embodiment.
Embodiment 1:
A kind of nano flame retardant polybutylene terephthalate material, its component by mass percent proportioning is: the compound 1% of polybutylene terephthalate 50%, alkali free glass fibre 20%, compound flame redundant 16%, acrylonitrile-butadiene-styrene copolymer (ABS) 8%, ethylene-methyl acrylate-glyceryl methacrylate terpolymer (E-MA-GMA) 4%, silane 0.2%, calcium stearate 0.8%, hindered phenol antioxygen 1076 and phosphite ester kind antioxidant 168.Described compound flame redundant is the compound that nano-sized magnesium hydroxide 30wt%, nano imvite 20wt% and polysilane fire retardant 50wt% three mix, wherein all silane modified processing of nano-sized magnesium hydroxide and nano imvite.
Preparation method: (1) is dried 3～5 hours by polybutylene terephthalate at 130 ℃～140 ℃, and moisture control is below 0.03%, stand-by; (2) alkali free glass fibre is dried to 3～6 hours at 80 ℃～110 ℃, take by weight ratio more dried alkali free glass fibre and silane, add together in the high-speed mixer of 3000～8000 revs/min, at the temperature that maintains 80 ℃～110 ℃, stir 10～60 minutes, make evenly coated alkali free glass fibre of silane, then be cooled to and make surface-treated alkali free glass fibre lower than 40 ℃, stand-by; (3) take by weight ratio nano imvite 20wt% and the polysilane fire retardant 50wt% of the nano-sized magnesium hydroxide 30wt% of silane modified processing, silane modified processing, make to mix, make compound flame redundant, then at 80 ℃～85 ℃, be dried 30～45 minutes, stand-by; (4) take by weight ratio polybutylene terephthalate, compound flame redundant and the alkali free glass fibre through silane surface treatment after drying treatment, after mixing, the compound that adds again the acrylonitrile-butadiene-styrene copolymer (ABS), ethylene-methyl acrylate-glyceryl methacrylate terpolymer (E-MA-GMA), calcium stearate and hindered phenol antioxygen 1076 and the phosphite ester kind antioxidant 168 that take by weight ratio, then adds together in high-speed mixer and fully mixes 10～30 minutes; (5) material again step (4) being mixed adds and in twin screw extruder, carries out abundant fusion plastification and mediate mixing, melt temperature is controlled at 190 ℃～250 ℃, after extruding by twin screw extruder, obtain nano flame retardant polybutylene terephthalate material of the present invention through overcooling, pelletizing, after dry.
Embodiment 2:
A kind of nano flame retardant polybutylene terephthalate material, its component by mass percent proportioning is: the compound 0.5% of polybutylene terephthalate 40%, nano-calcium carbonate 30%, compound flame redundant 20%, ethylene-vinyl acetate copolymer (EVA) 5%, maleic anhydride extension bar ethylene-octene copolymer (POE-g-MAH) 4%, Magnesium Stearate 0.2%, ethylene bis stearic amide 0.3%, hindered phenol antioxygen 1076 and phosphite ester kind antioxidant 168.Described compound flame redundant is the compound that nano-sized magnesium hydroxide 30wt%, nano imvite 20wt% and polysilane fire retardant 50wt% three mix, wherein all silane modified processing of nano-sized magnesium hydroxide and nano imvite.
Preparation method: (1) is dried 3～5 hours by polybutylene terephthalate at 130 ℃～140 ℃, and moisture control is below 0.03%, stand-by; (2) nano-calcium carbonate is dried to 3～6 hours at 80 ℃～110 ℃, take by weight ratio more dried nano-calcium carbonate and Magnesium Stearate, add together in the high-speed mixer of 3000～8000 revs/min, at the temperature that maintains 80 ℃～110 ℃, stir 10～60 minutes, make the even coated nano calcium carbonate of Magnesium Stearate, then be cooled to and make surface-treated nano-calcium carbonate lower than 40 ℃, stand-by; (3) take by weight ratio nano imvite 20wt% and the polysilane fire retardant 50wt% of the nano-sized magnesium hydroxide 30wt% of silane modified processing, silane modified processing, make to mix, make compound flame redundant, then at 80 ℃～85 ℃, be dried 30～45 minutes, stand-by; (4) take by weight ratio polybutylene terephthalate after drying treatment, compound flame redundant and through Magnesium Stearate surface-treated nano-calcium carbonate, after mixing, the compound that adds again the ethylene-vinyl acetate copolymer (EVA), maleic anhydride extension bar ethylene-octene copolymer (POE-g-MAH), ethylene bis stearic amide and hindered phenol antioxygen 1076 and the phosphite ester kind antioxidant 168 that take by weight ratio, then adds together in high-speed mixer and fully mixes 10～30 minutes; (5) material again step (4) being mixed adds and in twin screw extruder, carries out abundant fusion plastification and mediate mixing, melt temperature is controlled at 190 ℃～250 ℃, after extruding by twin screw extruder, obtain nano flame retardant polybutylene terephthalate material of the present invention through overcooling, pelletizing, after dry.
Embodiment 3:
A kind of nano flame retardant polybutylene terephthalate material, its component by mass percent proportioning is: the compound 0.5% of polybutylene terephthalate 60%, nano kaoline 20%, compound flame redundant 10%, MBS (MBS) 6%, maleic anhydride graft styrene-butadiene-styrene (SBS-g-MAH) 3%, phosphoesterase 30 .2%, ethylene bis stearic amide 0.3%, hindered phenol antioxygen 1076 and phosphite ester kind antioxidant 168.Described compound flame redundant is the compound that nano-sized magnesium hydroxide 30wt%, nano imvite 20wt% and polysilane fire retardant 50wt% three mix, wherein all silane modified processing of nano-sized magnesium hydroxide and nano imvite.
Preparation method: (1) is dried 3～5 hours by polybutylene terephthalate at 130 ℃～140 ℃, and moisture control is below 0.03%, stand-by; (2) nano kaoline is dried to 3～6 hours at 80 ℃～110 ℃, take by weight ratio more dried nano kaoline and phosphoric acid ester, add together in the high-speed mixer of 3000～8000 revs/min, at the temperature that maintains 80 ℃～110 ℃, stir 10～60 minutes, make the even clad nano kaolin of phosphoric acid ester, then be cooled to and make surface-treated nano kaoline lower than 40 ℃, stand-by; (3) take by weight ratio nano imvite 20wt% and the polysilane fire retardant 50wt% of the nano-sized magnesium hydroxide 30wt% of silane modified processing, silane modified processing, make to mix, make compound flame redundant, then at 80 ℃～85 ℃, be dried 30～45 minutes, stand-by; (4) take by weight ratio polybutylene terephthalate after drying treatment, compound flame redundant and through phosphoric acid ester surface-treated nano kaoline, after mixing, the compound that adds again the MBS (MBS), maleic anhydride graft styrene-butadiene-styrene (SBS-g-MAH), ethylene bis stearic amide and hindered phenol antioxygen 1076 and the phosphite ester kind antioxidant 168 that take by weight ratio, then adds together in high-speed mixer and fully mixes 10～30 minutes; (5) material again step (4) being mixed adds and in twin screw extruder, carries out abundant fusion plastification and mediate mixing, melt temperature is controlled at 190 ℃～250 ℃, after extruding by twin screw extruder, obtain nano flame retardant polybutylene terephthalate material of the present invention through overcooling, pelletizing, after dry.
Claims (9)
1. a nano flame retardant polybutylene terephthalate material, it is characterized in that, its component by mass percent proportioning is: polybutylene terephthalate 30%～60%, toughener 15%～30%, compound flame redundant 10%～20%, toughner 5%～10%, compatilizer 3%～5%, surface treatment agent 0.1%～0.5%, lubricant 0.1%～1%, oxidation inhibitor 0.1%～1%.
2. nano flame retardant polybutylene terephthalate material according to claim 1, is characterized in that, described toughener is the one in alkali free glass fibre, nano-calcium carbonate, nano kaoline, wollastonite, whisker.
3. nano flame retardant polybutylene terephthalate material according to claim 1, it is characterized in that, described compound flame redundant is the compound that nano-sized magnesium hydroxide 30wt%, nano imvite 20wt% and polysilane fire retardant 50wt% three mix, wherein all silane modified processing of nano-sized magnesium hydroxide and nano imvite.
4. nano flame retardant polybutylene terephthalate material according to claim 1, it is characterized in that, described toughner is the one in acrylonitrile-butadiene-styrene copolymer (ABS), ethylene-vinyl acetate copolymer (EVA), MBS (MBS).
5. nano flame retardant polybutylene terephthalate material according to claim 1, it is characterized in that, described compatilizer is the one in ethylene-methyl acrylate-glyceryl methacrylate terpolymer (E-MA-GMA), maleic anhydride grafted ethene-propylene-non-conjugated diene hydrocarbon copolymer (EPDM-g-MAH), maleic anhydride extension bar ethylene-octene copolymer (POE-g-MAH), maleic anhydride graft styrene-butadiene-styrene (SBS-g-MAH).
6. nano flame retardant polybutylene terephthalate material according to claim 1, is characterized in that, described surface treatment agent is the one in Magnesium Stearate, titanic acid ester, Aluminate, silane and phosphoric acid ester.
7. nano flame retardant polybutylene terephthalate material according to claim 1, is characterized in that, described lubricant is calcium stearate or ethylene bis stearic amide.
8. nano flame retardant polybutylene terephthalate material according to claim 1, is characterized in that, described oxidation inhibitor is the compound of hindered phenol antioxygen 1076 and phosphite ester kind antioxidant 168.
9. the preparation method of nano flame retardant polybutylene terephthalate material according to claim 1, is characterized in that, comprises the following steps:
(1) polybutylene terephthalate is dried to 3～5 hours at 130 ℃～140 ℃, moisture control is below 0.03%, stand-by;
(2) toughener is dried to 3～6 hours at 80 ℃～110 ℃, take by weight ratio more dried toughener and surface treatment agent, add together in the high-speed mixer of 3000～8000 revs/min, at the temperature that maintains 80 ℃～110 ℃, stir 10～60 minutes, make evenly coated toughener of surface treatment agent, then be cooled to and make surface-treated toughener lower than 40 ℃, stand-by;
(3) take by weight ratio nano imvite 20wt% and the polysilane fire retardant 50wt% of the nano-sized magnesium hydroxide 30wt% of silane modified processing, silane modified processing, make to mix, make compound flame redundant, then at 80 ℃～85 ℃, be dried 30～45 minutes, stand-by;
(4) take by weight ratio polybutylene terephthalate, compound flame redundant and the surface treated toughener after drying treatment, after mixing, add again the toughner, compatilizer, lubricant and the oxidation inhibitor that take by weight ratio, then add together in high-speed mixer and fully mix 10～30 minutes;
(5) material again step (4) being mixed adds and in twin screw extruder, carries out abundant fusion plastification and mediate mixing, melt temperature is controlled at 190 ℃～250 ℃, after extruding by twin screw extruder, obtain nano flame retardant polybutylene terephthalate material of the present invention through overcooling, pelletizing, after dry.
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| CN201210561523.4A CN103881320A (en) | 2012-12-21 | 2012-12-21 | Nanometer flame-retardant polybutylene telephthalate material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106967285A (en) * | 2017-04-12 | 2017-07-21 | 星威国际家居有限公司 | High tenacity fire retardation PC/PBT alloy material and preparation method |
| CN109467794A (en) * | 2018-09-30 | 2019-03-15 | 句容峰岭科技有限公司 | A kind of fire-retardant hardware plastic material and preparation method thereof |
| CN114031905A (en) * | 2021-12-08 | 2022-02-11 | 天津柯文实业股份有限公司 | Preparation method of impact-resistant halogen-free flame-retardant PBT (polybutylene terephthalate) material |
| CN114539731A (en) * | 2022-02-09 | 2022-05-27 | 佛山市鑫诚环保新材料有限公司 | Flame-retardant material and preparation method thereof |
-
2012
- 2012-12-21 CN CN201210561523.4A patent/CN103881320A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106967285A (en) * | 2017-04-12 | 2017-07-21 | 星威国际家居有限公司 | High tenacity fire retardation PC/PBT alloy material and preparation method |
| CN109467794A (en) * | 2018-09-30 | 2019-03-15 | 句容峰岭科技有限公司 | A kind of fire-retardant hardware plastic material and preparation method thereof |
| CN114031905A (en) * | 2021-12-08 | 2022-02-11 | 天津柯文实业股份有限公司 | Preparation method of impact-resistant halogen-free flame-retardant PBT (polybutylene terephthalate) material |
| CN114539731A (en) * | 2022-02-09 | 2022-05-27 | 佛山市鑫诚环保新材料有限公司 | Flame-retardant material and preparation method thereof |
| CN114539731B (en) * | 2022-02-09 | 2023-06-13 | 佛山市鑫诚环保新材料有限公司 | Flame-retardant material and preparation method thereof |
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Application publication date: 20140625 |